Browsing by Author "Sambolino, Annalisa"
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- Determination of phthalic acid esters and di(2-ethylhexyl) adipate in fish and squid using the ammonium formate version of the QuEChERS method combined with gas chromatography mass spectrometryPublication . Sambolino, Annalisa; Ortega-Zamora, Cecilia; González-Sálamo, Javier; Dinis, Ana; Cordeiro, Nereida; Canning-Clode, João; Hernández-Borges, JavierIn the present study, the ammonium formate version of the QuEChERS method, considered highly advantageous in relation to instrument maintenance and other issues, was applied for the first time to extract a group of twelve phthalic acid esters (PAEs, i.e. dipropyl phthalate, DPP; diisobutyl phthalate, DIBP; dibutyl phthalate, DBP; diisopentyl phthalate, DIPP; di-n-pentyl phthalate, DNPP; dihexyl phthalate, DHP; butyl benzyl phthalate, BBP; dicyclohexyl phthalate, DCHP; di(2-ethylhexyl) phthalate, DEHP; di-n-octyl phthalate, DNOP; diisononyl phthalate, DINP; and diisodecyl phthalate, DIDP) and one adipate (di(2-ethylhexyl) adipate, DEHA) from two species of fish (Scomber colias and Katsuwonus pelamis) and one of squid (Loligo gahi). The method was validated in terms of linearity, trueness and matrix effects. Determination coefficients (R2 ) for matrix-matched calibration curves were higher than 0.99 in all cases, being the lowest calibration levels in the range 0.5–10 ng/g. Mean recovery values were between 70 and 117% with relative standard deviation values ≤20%. Matrix effects were soft (between − 20 and +20%) for most analytes and matrices, except in squid samples, which was mostly medium with a moderate ion suppression. The analysis of 10 samples of each type showed the presence of DIBP, DBP and DEHP at concentrations up to 44.2 ± 2.1 ng/g of wet weight in some of the samples and species, still not representing concerning values when considering the daily intake of such species of seafood in the human diet (tolerable daily intake -TDI- values were not exceeded). Results demonstrated that the ammonium formate version of the QuEChERS method can be applied with success for the extraction and determination of the selected PAEs and DEHA in fish and squid samples.
- Microplastic ingestion and plastic additive detection in pelagic squid and fish: implications for bioindicators and plastic tracers in open oceanic food websPublication . Sambolino, Annalisa; Iniguez, Eva; Herrera, Inma; Kaufmann, Manfred ; Dinis, Ana; Cordeiro, Nereida ; Sambolino, Annalisa; Iñiguez Santamaría, Eva; Kaufmann, Manfred; cordeiro, nereidaThe ubiquitous presence of microplastics (MPs) in the ocean represents a potential threat to marine organisms, with poorly understood long-term adverse effects, including exposure to plastic additives. The present study investigated the ingestion of MPs in two epipelagic fish species (Trachurus picturatus and Scomber colias) and three pelagic squid spe cies (Loligo vulgaris, Ommastrephes caroli and Sthenoteuthis pteropus) from an open oceanic region of the Northeast Atlan tic. Seven phthalate esters (PAEs) were also analysed in the organisms' tissue, and the potential correlation between PAEs concentrations and ingested MPs was investigated. Seventy-two fish and 20 squid specimens were collected and analysed. MPs were found in the digestive tract of all species and in the squid species' gills and ink sacs. The highest occurrence of MPs was in the stomach of S. colias (85 %) and the lowest in the stomach and ink sac of O. caroli and L. vulgaris (12 %). Most of the particles identified (>90 %) were fibres. Among all the ecological and biological factors considered (dietary preferences, season, body size, total weight, liver weight, hepatosomatic index and gastrosomatic index), only gastrosomatic index (GSI) and season were significant predictors of MPs ingestion in fish species, with a greater likelihood of ingestion in the cold season and in specimens with higher GSI values (i.e. higher feeding inten sity). Four PAEs (DEP, DIBP, BBP, DEHP) were detected in all the species analysed, with average ∑PAEs concentrations ranging between 10.31 and 30.86 ng/g (wet weight). DIBP was positively correlated with ingested MPs, suggesting this compound might represent a “plastic tracer”. This study looks into the problem of MPs ingestion for pelagic species in an open oceanic region, highlighting the most suitable bioindicators and providing essential insights into the factors that may influence ingestion rates. Additionally, the detection of PAEs in all species indicates the need for further re search on the contamination sources, the effects of these chemicals on marine organisms, and the potential risks to human health through seafood consumption.
- Optimization and validation of a micro–QuEChERS method for phthalates detection in small samples of cetacean blubberPublication . Sambolino, Annalisa; Rodriguez, Marta; De la Fuente, Jesus; Arbelo, Manuel; Fernández, Antonio; Kaufmann, Manfred; Cordeiro, Nereida; Dinis, AnaIn this study, an innovative method was developed to detect and quantify phthalates in fresh cetacean blubber. An adaptation of the ammonium formate QuEChERS method was used and adapted as a micro-extraction for small quantities of samples. Significantly, this technique utilized minimal quantities of reagents and salts, with the additional implementation of rigorous Quality Assurance/Quality Control protocols to further reduce background contamination. To ensure the reliability of this method, comprehensive validation procedures were conducted, with a specific focus on two widely studied cetacean species: the common bottlenose dolphin (Tursiops truncatus) and the short-finned pilot whale (Globicephala macrorhynchus). Determination coefficients (R2) for matrix-matched calibration were >0.93 with limits of quantifications (LOQ) of the method in the range of 5–10 ng/g. Mean recovery values were between 40 and 100 %. This novel methodology holds particular relevance for environmental research studies, offering the capability to detect emerging contaminants with minimal sample requirements. This aspect is particularly valuable in investigations that involve free-ranging animals and rely on biopsy sampling. It allows for the assessment of contaminant levels in healthy individuals within wild populations, enhancing our understanding of ecological impacts and potential conservation measures. • A micro-extraction adaptation of the ammonium formate QuEChERS method was developed and applied to a small quantity of fresh cetacean blubber to detect phthalates. • Small quantities of reagents and salts were used, and additional Quality Assurance/ Quality Control procedures were taken to further minimize background contamination. • Method validation was carried out for two cosmopolitan and extensively studied cetacean species: the common bottlenose dolphin (Tursiops truncatus) and the short-finned pilot whale (Globicephala macrorhynchus).
- Phthalates as plastic tracers in a pelagic food web from an open oceanic environmentPublication . Sambolino, Annalisa; Cordeiro, Nereida Maria Abano; Kaufmann, Manfred Josef; Dinis, Ana Margarida Brites CaetanoA investigação científica nas ciências ambientais e biológicas preocupa-se cada vez mais dos efeitos adversos das atividades humanas. A poluição por plásticos tem recebido atenção global devido ao seu evidente impacto ambiental, especialmente nos ecossistemas marinhos. Os microplásticos (MPs), definidos como partículas de plástico com menos de 5 mm, são de particular preocupação devido à sua persistência e capacidade de se infiltrar nas cadeias alimentares. No entanto, o ambiente pelágico continua a ser um dos ambientes menos explorados e mais desafiantes para estudar. Este estudo teve como objetivo investigar a presença de microplásticos numa cadeia alimentar pelágica num ecossistema oceânico, examinando em simultâneo a ocorrência de aditivos plásticos, especificamente os ftalatos (PAEs), como potenciais “tracers”. A amostragem ao longo de um ano das águas superficiais ao redor de uma ilha oceânica revelou uma presença consistente de MPs, especialmente microfibras, com flutuações sazonais significativas na razão entre MPs e zooplâncton. A análise do conteúdo estomacal das espécies de peixes pelágicos e lulas mais prevalentes que habitam estas águas confirmou que a maioria dos indivíduos ingeriu MPs, e foi observada uma correlação entre a abundância de MPs e a concentração de PAEs, particularmente DIBP (di isobutyl phthalate), nos seus tecidos. A análise de PAEs em amostras de biópsia de cetáceos que se alimentam destas presas, revelou uma presença persistente e alarmantemente elevada destes aditivos plásticos. Isso sugere uma exposição crônica e duradoura, provavelmente por meio de transferência trófica. A utilização de indicadores indiretos, como os aditivos plásticos, revela-se de grande importância em ambientes de difícil acesso e investigação, especialmente ao estudar animais protegidos, como a megafauna marinha, na qual as amostras são limitadas e de difícil obtenção. Neste estudo, foram desenvolvidas e validadas metodologias inovadoras para a deteção e quantificação de PAEs em biota marinho. A deteção de MPs e PAEs em vários níveis desta teia trófica oceanopelágica destaca a presença generalizada destes contaminantes antropogénicos mesmo em regiões oceânicas remotas.
- Seasonal variation in microplastics and zooplankton abundances and characteristics: the ecological vulnerability of an oceanic island systemPublication . Sambolino, Annalisa; Herrera, Inma; Álvarez, Soledad; Rosa, Alexandra; Alves, Filipe; Canning-Clode, João; Cordeiro, Nereida; Dinis, Ana; Kaufmann, ManfredThe ingestion of microplastics (MPs - plastic particles <5 mm) by planktivorous organisms represents a signif icant threat to marine food webs. To investigate how seasonality might affect plastic intake in oceanic islands' ecosystems, relative abundances and composition of MPs and mesozooplankton samples collected off Madeira Island (NE Atlantic) between February 2019 and January 2020 were analysed. MPs were found in all samples, with fibres accounting for 89 % of the particles. MPs and zooplankton mean abundance was 0.262 items/m3 and 18.137 individuals/m3 , respectively. Their monthly variations follow the seasonal fluctuation of environmental parameters, such as currents, chlorophyll-a concentration, sea surface temperature and precipitation intensity. A higher MPs/zooplankton ratio was recorded in the warm season (May-Oct), reaching 0.068 items/individual when considering large-sized particles (1000–5000 μm). This is the first study to assess the seasonal variability of MPs in an oceanic island system providing essential information respecting its ecological impact in pelagic environments.